Nuclear magnetic resonance (NMR) spectroscopy is considered the “gold-standard” for structure characterization of small molecules and proteins because of its inherent sensitivity to structural changes, atomic resolution, and quantitative nature. A resurgence of research in peptides and oligonucleotides (TIDES) has brought NMR at the forefront of analytical techniques for characterizing these modalities. Recent advancements in NMR technology accelerate the development and characterization of novel therapeutic TIDES and generic products.